反应 #62356

反应方程式

trityl chloride

5-iodo-3-(naphthalen-2-yl)-1H-thieno[2,3-c]pyrazole

N,N-dimethylformamide

1H-Thieno[2,3-c]pyrazole-5-carbonitrile

sodium hydride

→

title compound

收率 75.4%

5-Iodo-3-(naphthalen-2-yl)-1-trityl-1H-thieno[2,3-c]-pyrazole

收率 75.4%

溶剂

water

ethyl acetate

反应条件

后处理

1. 1
   workup.STIRRINGstirred at this temperature for a day
2. 2
   洗涤the organic layer was washed successively with saturated aqueous ammonium chloride and saturated brine
3. 3
   干燥dried over anhydrous magnesium sulfate
4. 4
   其他the solvent was evaporated
5. 5
   其他The residue was purified
6. 6
   其他separated by silica gel column chromatography (ethyl acetate:n-hexane=1:30)

实验过程

To a solution of 75 mg of 5-iodo-3-(naphthalen-2-yl)-1H-thieno[2,3-c]pyrazole in 1 m L of N,N-dimethylformamide 1 was added 12 mg of sodium hydride at room temperature, stirred for 15 minutes, then added with 56 mg of trityl chloride, and stirred at this temperature for a day. The solution was added with water and diluted with ethyl acetate, and the organic layer was washed successively with saturated aqueous ammonium chloride and saturated brine, dried over anhydrous magnesium sulfate, and the solvent was evaporated. The residue was purified and separated by silica gel column chromatography (ethyl acetate:n-hexane=1:30), to afford 93 mg of the title compound as colorless crystals.

来源